Process of making thorium sulfid.



J. L. HUBER. PROCESS 0F MAKING THORIUM SULFID. APPLIoATIoN FILED' JUNE 1, 1908.

94h71 o Patented NQV.`23, 1909.

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JOHANN LUDI'IG HUBER, OF NIEDERSCHNEVJEIDE, NEAR BERLIN, GERMANY, .AS- SIGNOR TO THE FIR-IVI OF K'UNHEIII U. CO., OF NIEDERSCHNEWEIDE, NEAR BER- LIN, GERBTANY.

PROCESS 0F BIAKING THORIUIVI SULFID.

T 0 all whom it may concern.'

Be it known that I, JOHANN LUDWIG HU- BER, doctor of philosophy, chemist, a subject of the Grand Duke vof Baden and the German Emperor, residing at Niederschne- Weide, near Berlin, Germany, have invented new and useful Improvements in Processes of Making Thorium Sulfid, of which the following is a specification.

The suld of thorium is a very suitable material for producing thorium metal usable in iilaments for electric incandescentlamps.

I have discovered that one can prepare easily sulfid of thorium in a very pure state, especially free from carbon by treating the dry halogen compounds of thorium, especially the chlorid of thorium, with dry sulfureted hydrogen, free from air, at a temperature below the sublimation temperature of the halogen compound of thorium, but as near to that temperature as possible. I have found that a very suitable temperature for conducting my process is at about 550 C. The sulfureted hydrogen is led over the heated halogen compound of thorium in a slow stream. I have found it as suitable to add to the halogen compound of thorium substances which are not attacked by the halogen compound of thorium nor by the sulfureted hydrogen. The purpose of such additions is to avoid a conglomeration of the halogen compound or the obtained sultid of thorium and to moderate the reaction. I may use as additions for example: infusorial earth, asbestos, clay. IVhen using these materials it is diiiicult to separate the additions from the obtained suliid of thorium. If I desire to obtain pure sultid of thorium I use as additions substances which may be easily separated from the sulfd of thorium. I may use chlorid of potassium or sodium. I may employ a mixture of chlorid of thorium with 5, l0, or any amount up to per cent. of chlorid of potassium. The proportion of the chlorid of potassium depends on the velocity with which I wish to conduct the reaction. It I desire to finish with the reaction in a short time, I use a smaller pro- Specication of Letters Patent.

Application filed June 1, 190g.

Patented Nov. 23, 1909.

serial No. 436,120.

portion of addition than if I desire to moderate the reaction in a higher degree. The separation of the chlorid of sodium from the sulfid of thorium is effected by lixiviating the product of the reaction with water and iiltering off the undissolved sultid of thorium from the liquid.

rIhe sulfureted hydrogen may be used in a pure state or mixed with inert gases, for example nitrogen or carbonio acid.

In the drawing a vertical section through an apparatus suitable for carrying out my process is shown.

a is a tube containing haloid of thorium. At Z) the sulfureted hydrogen is introduced and at c the gases are led away.

CZ is a suitable heating means.

Sulfureted hydrogen is conducted over the haloid of thorium until the gases leaving tube a will be free of hydrohaloid acid.

What I claim as my invention and desire to secure by Letters Patent, is:

l. The process of making thorium sulfid which consists in causing sulfureted hydrogen to react on heated haloid of thorium in a solid state at temperatures below the sublimation temperature of haloid of thorium.

2. The process of making thorium sulfid which consists in causing sulfureted hydrogen to react on heated haloid of thorium in a solid state mixed with substances indifferent to haloid of thorium and sulfureted hydrogen below the sublimation temperature of haloid of thorium.

3. The process of making thorium suliid which consists in causing sulfureted hydrogen to react on heated chlorid of thorium in a solid state mixed with chlorid of sodium below the sublimation temperature of chlorid ot thorium.

In testimony whereof I have signed my name to this specification in the presence of two subscribing witnesses.

JOHANN LUDIIG HUBER.

Witnesses HENRY HASPER, VVOLDEMAR HAUPT. 

